Hydrochloric Acid → HCID 72740628, Verbindung

HRID 507063

Reaktionsgleichung

Reaktionsgleichung von HRID 507063
Cl[C:2](Cl)(Cl)[CH:3]([OH:5])O.S([O-])([O-])(=O)=O.[Na+].[Na+].S(O)(O)(=O)=O.[NH2:20][OH:21].[NH2:22][C:23]1[CH:31]=[CH:30][CH:29]=[C:28]2[C:24]=1[CH2:25][CH2:26][CH2:27]2.Cl>O>[OH:21][N:20]=[CH:2][C:3]([NH:22][C:23]1[CH:31]=[CH:30][CH:29]=[C:28]2[C:24]=1[CH2:25][CH2:26][CH2:27]2)=[O:5]

Komponenten

7

Edukt 5

HCID 313Hydrochloric AcidHCID 2707Chloral HydrateHCID 24436Sodium SulfateHCID 1225694-AminoindanHCID 159255Hydroxylamine, sulfate (1:1)

Produkt 1

HCID 72740628HCID 72740628, VerbindungAusbeute 90,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Reaktionsbedingungen

Temperatur
45 °C

Versuchsvorschrift

To a solution of chloral hydrate (5.46 g, 33 mmol) and anhydrous sodium sulfate (25.6 g, 180 mmol) in water (92 mL) add a mixture of hydroxylamine sulfate (25.6 g, 156 mmol), 4-aminoindane (4 g, 30 mmol), concentrated hydrochloric acid (3.1 mL) in water (30.8 mL). Heat the mixture up to 45° C. for 90 min, to 52° C. over 45 min and to 75° C. for 60 min. Cool the mixture to room temperature and filter the solid. Wash the solid with water and hexane. Dry the solid under vacuum to yield the title compound (5.54 g, 90%). MS (ES−): 203 (M−H).

Aufarbeitung

  1. waitto 75° C. for 60 min
  2. temperatureCool the mixture to room temperature
  3. filtrationfilter the solid
  4. washWash the solid with water and hexane
  5. customDry the solid under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-5698eb4ae42646b0a98745a51caaad1c
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07786108B2

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